EuCO 3 OH microspheres have been successfully prepared using a facile hydrothermal approach, by using urea as the precipitant without the assistance of any surfactants or templates. Several experimental parameters were examined, such as the reaction temperature, the reaction time, and the molar ratios of the starting reagents. The Eu 2 O 3 microspheres have been prepared by thermal conversion of EuCO 3 OH microspheres at 800 °C in air for 6 h. The as-obtained products were characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, thermogravimetrydifferential thermal analysis and photoluminescence. The possible growth process for the EuCO 3 OH microspheres was discussed.